CN111266120A - CdS/ZnO composite photocatalytic material with hollow structure and preparation method thereof - Google Patents
CdS/ZnO composite photocatalytic material with hollow structure and preparation method thereof Download PDFInfo
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract
The invention relates to a CdS/ZnO composite photocatalytic material with a hollow structure and a preparation method thereof, which comprises the steps of uniformly mixing a zinc acetate aqueous solution and a sodium hydroxide solution to obtain a mixed solution A, carrying out water-bath heating reaction treatment on the mixed solution A, and carrying out post-treatment after the water-bath heating reaction is finished to obtain ZnO nano powder; and ultrasonically dispersing ZnO nano powder into a cadmium acetate aqueous solution to obtain a dispersion liquid A, adding a thiourea solution into the dispersion liquid A, uniformly mixing to obtain a mixed liquid B, carrying out water bath heating reaction treatment on the mixed liquid B, and carrying out post-treatment after the water bath heating reaction is finished to obtain the CdS/ZnO composite photocatalytic material with the hollow structure. The CdS/ZnO composite photocatalytic material with the hollow structure prepared by the invention is a semiconductor composite metal compound, has huge application prospects in the aspects of photoelectrocatalysis, optical materials, gas sensitivity and the like, does not adopt an organic solvent in the preparation process, is green, environment-friendly and energy-saving, has easily obtained raw materials, low cost and simple instruments, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of composite nano-material preparation, in particular to a CdS/ZnO composite photocatalytic material with a hollow structure and a preparation method thereof.
Background
ZnO has the characteristics of wide forbidden band width (3.37 eV), high photocatalytic efficiency, low price, environmental friendliness and the like, so that ZnO occupies an important position in the research of photocatalytic degradation of organic pollutants. Since ZnO is a direct band gap semiconductor, it is better than TiO2The method has higher quantum efficiency, and more oxygen vacancies exist on the surface of ZnO, so that sufficient conditions are provided for the formation of electron traps, the recombination time of electrons and holes can be prolonged, and the photocatalytic activity is further improved. But has the disadvantages that: the absorption range of ZnO is narrow, and the ZnO is only limited to the ultraviolet region, so that the further development and application of ZnO in the field of photocatalysis are limited.
CdS is a narrow band gap semiconductor and has wide application in the fields of photoelectric conversion and photocatalysis. As an excellent photocatalyst, CdS can effectively degrade most organic matters in chemical wastewater, and plays a good role in wastewater treatment and environmental protection, but CdS is easily oxidized by photo-generated holes during photocatalytic reaction and is corroded by light so as to lose activity. As the band gap of CdS is smaller than that of ZnO, CdS nano-particles are modified on the surface of ZnO to obtain a ZnO/CdS composite structure, the band gap of a semiconductor is widened, and the recombination probability of photo-generated electron-hole pairs is reduced, so that the photo-catalytic activity is improved, and the method has potential application in the aspects of photo-catalytic degradation of organic pollutants, photo-water splitting for hydrogen production and the like.
In recent years, scientists have made some exploratory work on the controlled synthesis of CdS/ZnO composite nano-materials and also have made some results. Kim et al prepared a microspherical ZnO/CdS core-shell structure (ceramics International, 2017, 43, 13493-13499) by a chemical precipitation method. Chen et al obtained CdS-ZnO core-shell nanowires (Nano Energy, 2018, 43, 270-277) by a physical synthesis technology. Wang et al synthesized ZnO-CdS core-shell nanorods by a two-step method (International Journal of Hydrogen Energy,2010, 35, 8199-8205). Mahala obtains ZnO nano-sheets through electrochemical deposition, and then CdS nano-particles are loaded on the surfaces of the ZnO nano-sheets (New Journal of chemistry, 2019, 43, 7001-. Chen et al obtained ZnO/CdS core-shell nanowires on a silicon substrate through a two-step ion exchange path (Surface & Coatings Technology, 2017, 320, 467-. Yang et al firstly adopts a hydrothermal technology to grow a ZnO nanorod, and then CdS is deposited on the surface of the ZnO nanorod by pulse laser to obtain a ZnO/CdS core-shell nanorod (Applied Physics Letters, 2016, 109, 203106).
According to research and research of documents, the CdS/ZnO composite photocatalytic material with a hollow structure prepared by adopting a simple water bath chemical synthesis technology is not reported.
Disclosure of Invention
The invention aims to provide a CdS/ZnO composite photocatalytic material with a hollow structure and a preparation method thereof, so as to fill the blank of the prior art and add a new variety to a ZnO-CdS composite nano-structured material.
The technical scheme adopted by the invention is as follows:
a CdS/ZnO composite photocatalytic material with a hollow structure is characterized in that: the CdS/ZnO composite photocatalytic material mainly has a hollow one-dimensional nano-tube structure, a hollow flower-shaped structure assembled by a small number of one-dimensional nano-tube structures exists, the diameter of each nano-tube is 50-100nm, the length of each nano-tube is 2.0-4.0 microns, the substrate of the CdS/ZnO composite photocatalytic material is a ZnO crystal, and granular CdS nano-crystals are distributed on the surface of the ZnO crystal.
A preparation method of a CdS/ZnO composite photocatalytic material with a hollow structure is characterized by comprising the following operation steps:
s1: uniformly mixing a zinc acetate aqueous solution and a sodium hydroxide solution to obtain a mixed solution A, carrying out water-bath heating reaction treatment on the mixed solution A, and carrying out post-treatment after the water-bath heating reaction is finished to obtain ZnO nano powder;
s2: and ultrasonically dispersing ZnO nano powder into a cadmium acetate aqueous solution to obtain a dispersion liquid A, adding a thiourea solution into the dispersion liquid A, uniformly mixing to obtain a mixed liquid B, carrying out water bath heating reaction treatment on the mixed liquid B, and carrying out post-treatment after the water bath heating reaction is finished to obtain the CdS/ZnO composite photocatalytic material with the hollow structure.
Specifically, the method comprises the following steps: the molar ratio of the zinc acetate to the sodium hydroxide in the mixed solution A is 1: 30; adding 0.04-0.08 g of ZnO nano powder into every 0.2-1.0 mmol of cadmium acetate in the dispersion liquid A for ultrasonic dispersion; 0.8-1.5 mmol of thiourea is added into every 0.2-1.0 mmol of cadmium acetate in the mixed solution B.
The temperature of the water bath heating reaction treatment in the step S1 is 90 ℃, and the time is 4 h; step S2, the temperature of the water bath heating reaction treatment is 90 ℃, and the time is 3-5 h; in the step S2, the ultrasonic dispersion time is 30-40 min.
Preferably: adding 0.05g of ZnO nano powder into every 0.4mmol of cadmium acetate in the dispersion liquid A for ultrasonic dispersion; and adding 1.0mmol of thiourea into every 0.4mmol of cadmium acetate in the mixed solution B.
The CdS/ZnO composite photocatalytic material with the hollow structure prepared by the invention is a semiconductor composite metal compound, has huge application prospects in the aspects of photoelectrocatalysis, optical materials, gas sensitivity and the like, does not adopt an organic solvent in the preparation process, is green, environment-friendly and energy-saving, has easily obtained raw materials, low cost and simple instruments, and is suitable for industrial production.
Drawings
FIG. 1 is an X-ray diffraction (XRD) diagram of a CdS/ZnO composite photocatalytic material with a hollow structure;
FIG. 2 is a Scanning Electron Microscope (SEM) picture of a CdS/ZnO composite photocatalytic material with a hollow structure;
FIG. 3 is a Scanning Electron Microscope (SEM) picture of a CdS/ZnO composite photocatalytic material with hollow structures;
FIG. 4 is a comparison graph of the effect of the CdS/ZnO composite photocatalytic material of the present invention on degradation of organic dye, malachite green, with pure CdS and ZnO.
Detailed Description
The technical solution of the present invention is further fully described in detail by the following specific examples. The following examples are further illustrative of the present invention and do not limit the scope of the present invention.
Example 1
The technical scheme of the invention is to prepare the CdS/ZnO composite photocatalytic material with a hollow structure by adopting a water bath chemical synthesis technology, and the specific process flow is as follows:
(1) 30mL of a solution containing 1mmol of zinc acetate (Zn (CH)3COO)2·2H2O) ofMagnetic stirring is carried out on the aqueous solution and 30mL of aqueous solution dissolved with 30mmol of sodium hydroxide (NaOH) for 30 minutes;
(2) placing the reaction mixed solution in a water bath kettle, setting the temperature to be 90 ℃, reacting for 4 hours, naturally cooling to room temperature, carrying out suction filtration, washing and drying to obtain ZnO nano powder;
(3) 0.05g of ZnO nanopowder was weighed and added to 30mL of cadmium acetate (Cd (CH) containing 0.4mmol3COO)2·2H2O) in the water solution, performing ultrasonic dispersion for 30 minutes to obtain a dispersion liquid A;
(4) weighing 1mmol of thiourea, adding 30mL of deionized water, and dissolving to obtain a solution B;
(5) adding the solution B into the dispersion liquid A, continuously stirring for 30 minutes, placing the reaction mixed liquid into a water bath kettle, setting the temperature to be 90 ℃, and reacting for 4 hours;
(6) and after the reaction is finished, naturally cooling to room temperature, carrying out suction filtration on the precipitate, washing the precipitate with absolute ethyl alcohol and distilled water for 3-5 times respectively, and drying the precipitate in a vacuum drying oven for 8 hours at the temperature of 60 ℃ to obtain the CdS/ZnO composite photocatalytic material with the hollow structure.
Referring to the attached figure 1, the X-ray diffraction (XRD) pattern of the CdS/ZnO composite photocatalytic material with the hollow structure prepared by the method in the example 1 is compared with a JCPDS standard card, diffraction peaks appearing in the pattern can be respectively marked as hexagonal phase ZnO (with the card number of 36-1451) and hexagonal phase CdS (with the card number of 41-1049), and no other impurity peaks exist. XRD shows that the prepared product is CdS/ZnO compound.
Referring to the attached figure 2, a Scanning Electron Microscope (SEM) picture of the CdS/ZnO composite photocatalytic material with the hollow structure prepared by the method in the embodiment 1 shows that the product mainly has a hollow one-dimensional tubular structure, a hollow flower-shaped structure assembled by a few one-dimensional structures exists, the diameter of a nanotube is 50-100nm, and the length of the nanotube is 2.0-4.0 microns. The lower right inset clearly shows the features of the hollow structure.
Referring to fig. 3, a Scanning Electron Microscope (SEM) photograph of the CdS/ZnO composite photocatalytic material with a hollow structure prepared by the method described in example 1 shows a hollow three-dimensional flower-like structure, wherein the substrate of the composite is ZnO, and granular CdS nanocrystals are distributed on the surface of ZnO crystals.
Referring to the attached figure 4, the comparison graph of the effect of the CdS/ZnO composite photocatalytic material with a hollow structure prepared by the method in example 1 and the effect of pure CdS and ZnO in degrading organic dye malachite green (experimental conditions: xenon lamp light source (300W, lambda is more than or equal to 400 nm), catalyst 10mg and 50mL of aqueous solution containing 10mg/L of malachite green) is shown. As can be seen from FIG. 4, the prepared CdS/ZnO composite photocatalytic material has a photocatalytic degradation efficiency for malachite green in simulated wastewater that is significantly higher than that of pure CdS and pure ZnO, and shows excellent visible light catalytic activity.
Example 2
The technical scheme of the invention is to prepare the CdS/ZnO composite photocatalytic material with a hollow structure by adopting a water bath chemical synthesis technology, and the specific process flow is as follows:
(1) 30mL of a solution containing 1mmol of zinc acetate (Zn (CH)3COO)2·2H2O) and 30mL of an aqueous solution in which 30mmol of sodium hydroxide (NaOH) is dissolved, and magnetically stirring for 30 minutes;
(2) placing the reaction mixed solution in a water bath kettle, setting the temperature to be 90 ℃, reacting for 4 hours, naturally cooling to room temperature, carrying out suction filtration, washing and drying to obtain ZnO nano powder;
(3) 0.08g of ZnO nanopowder was weighed and added to 30mL of cadmium acetate (Cd (CH) containing 0.8mmol3COO)2·2H2O) in the water solution, ultrasonically dispersing for 40 minutes to obtain dispersion A;
(4) weighing 1.5mmol of thiourea, adding 30mL of deionized water, and dissolving to obtain a solution B;
(5) adding the solution B into the dispersion liquid A, continuously stirring for 35 minutes, placing the reaction mixed liquid into a water bath kettle, setting the temperature to be 90 ℃, and reacting for 5 hours;
(6) and after the reaction is finished, naturally cooling to room temperature, carrying out suction filtration on the precipitate, washing the precipitate with absolute ethyl alcohol and distilled water for 3-5 times respectively, and drying the precipitate in a vacuum drying oven for 10 hours at the temperature of 50 ℃ to obtain the CdS/ZnO composite photocatalytic material with the hollow structure.
Through XRD and SEM detection, the CdS/ZnO composite photocatalytic material with a hollow structure is prepared by the method described in the embodiment 2.
Example 3
The technical scheme of the invention is to prepare the CdS/ZnO composite photocatalytic material with a hollow structure by adopting a water bath chemical synthesis technology, and the specific process flow is as follows:
(1) 30mL of a solution containing 1mmol of zinc acetate (Zn (CH)3COO)2·2H2O) and 30mL of an aqueous solution in which 30mmol of sodium hydroxide (NaOH) is dissolved, and magnetically stirring for 30 minutes;
(2) placing the reaction mixed solution in a water bath kettle, setting the temperature to be 90 ℃, reacting for 4 hours, naturally cooling to room temperature, carrying out suction filtration, washing and drying to obtain ZnO nano powder;
(3) 0.06g of ZnO nanopowder was weighed and added to 30mL of cadmium acetate (Cd (CH) containing 0.6mmol3COO)2·2H2O) in the water solution, ultrasonically dispersing for 35 minutes to obtain a dispersion liquid A;
(4) weighing 1.2mmol of thiourea, adding 30mL of deionized water, and dissolving to obtain a solution B;
(5) adding the solution B into the dispersion liquid A, continuously stirring for 25 minutes, placing the reaction mixed liquid into a water bath kettle, setting the temperature to be 90 ℃, and reacting for 3 hours;
(6) and after the reaction is finished, naturally cooling to room temperature, carrying out suction filtration on the precipitate, washing the precipitate with absolute ethyl alcohol and distilled water for 3-5 times respectively, and drying the precipitate in a vacuum drying oven for 6 hours at the temperature of 60 ℃ to obtain the CdS/ZnO composite photocatalytic material with the hollow structure.
Through XRD and SEM detection, the CdS/ZnO composite photocatalytic material with a hollow structure is prepared by the method described in the embodiment 3.
Example 4
The technical scheme of the invention is to prepare the CdS/ZnO composite photocatalytic material with a hollow structure by adopting a water bath chemical synthesis technology, and the specific process flow is as follows:
(1) 30mL of a solution containing 1mmol of zinc acetate (Zn (CH)3COO)2·2H2O) and 30mL of an aqueous solution in which 30mmol of sodium hydroxide (NaOH) is dissolved, and magnetically stirring for 30 minutes;
(2) placing the reaction mixed solution in a water bath kettle, setting the temperature to be 90 ℃, reacting for 4 hours, naturally cooling to room temperature, carrying out suction filtration, washing and drying to obtain ZnO nano powder;
(3) 0.05g of ZnO nanopowder was weighed and added to 30mL of cadmium acetate (Cd (CH) containing 0.2mmol3COO)2·2H2O) in the water solution, ultrasonically dispersing for 40 minutes to obtain dispersion A;
(4) weighing 0.8mmol of thiourea, adding 30mL of deionized water, and dissolving to obtain a solution B;
(5) adding the solution B into the dispersion liquid A, continuously stirring for 30 minutes, placing the reaction mixed liquid into a water bath kettle, setting the temperature to be 90 ℃, and reacting for 5 hours;
(6) and after the reaction is finished, naturally cooling to room temperature, carrying out suction filtration on the precipitate, washing the precipitate with absolute ethyl alcohol and distilled water for 3-5 times respectively, and drying the precipitate in a vacuum drying oven for 8 hours at the temperature of 50 ℃ to obtain the CdS/ZnO composite photocatalytic material with the hollow structure.
Through XRD and SEM detection, the CdS/ZnO composite photocatalytic material with a hollow structure is prepared by the method described in the embodiment 4.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention. Structures, devices, and methods of operation not specifically described or illustrated herein are generally practiced in the art without specific recitation or limitation.
Claims (10)
1. A CdS/ZnO composite photocatalytic material with a hollow structure is characterized in that: the CdS/ZnO composite photocatalytic material mainly has a hollow one-dimensional nano-tube structure, a hollow flower-shaped structure assembled by a small number of one-dimensional nano-tube structures exists, the diameter of each nano-tube is 50-100nm, the length of each nano-tube is 2.0-4.0 microns, the substrate of the CdS/ZnO composite photocatalytic material is a ZnO crystal, and granular CdS nano-crystals are distributed on the surface of the ZnO crystal.
2. A preparation method of a CdS/ZnO composite photocatalytic material with a hollow structure is characterized by comprising the following operation steps:
s1: uniformly mixing a zinc acetate aqueous solution and a sodium hydroxide solution to obtain a mixed solution A, carrying out water-bath heating reaction treatment on the mixed solution A, and carrying out post-treatment after the water-bath heating reaction is finished to obtain ZnO nano powder;
s2: and ultrasonically dispersing ZnO nano powder into a cadmium acetate aqueous solution to obtain a dispersion liquid A, adding a thiourea solution into the dispersion liquid A, uniformly mixing to obtain a mixed liquid B, carrying out water bath heating reaction treatment on the mixed liquid B, and carrying out post-treatment after the water bath heating reaction is finished to obtain the CdS/ZnO composite photocatalytic material with the hollow structure.
3. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure according to claim 1, wherein the preparation method comprises the following steps: the molar ratio of the zinc acetate to the sodium hydroxide in the mixed solution A is 1: 30.
4. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure according to claim 1, wherein the preparation method comprises the following steps: the temperature of the water bath heating reaction treatment in the step S1 is 90 ℃, and the time is 4 h.
5. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure according to claim 1, wherein the preparation method comprises the following steps: 0.04-0.08 g of ZnO nano powder is added into every 0.2-1.0 mmol of cadmium acetate in the dispersion liquid A for ultrasonic dispersion.
6. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure according to claim 1, wherein the preparation method comprises the following steps: 0.8-1.5 mmol of thiourea is added into every 0.2-1.0 mmol of cadmium acetate in the mixed solution B.
7. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure according to claim 1, wherein the preparation method comprises the following steps: and S2, the temperature of the water bath heating reaction treatment is 90 ℃, and the time is 3-5 h.
8. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure according to claim 1, wherein the preparation method comprises the following steps: in the step S2, the ultrasonic dispersion time is 30-40 min.
9. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure, according to claim 5, is characterized in that: 0.05g of ZnO nano powder is added into every 0.4mmol of cadmium acetate in the dispersion liquid A for ultrasonic dispersion.
10. The preparation method of the CdS/ZnO composite photocatalytic material with the hollow structure, according to claim 6, is characterized in that: and adding 1.0mmol of thiourea into every 0.4mmol of cadmium acetate in the mixed solution B.
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